# Supplementary Material (ESI) for New Journal of Chemistry # This journal is (c) The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2006 data_global _journal_coden_Cambridge 440 loop_ _publ_author_name 'Marc Fourmigue' 'Olivier Jeannin' _publ_contact_author_name 'Marc Fourmigue' _publ_contact_author_address ; Sciences Chimiques de Rennes UMR 6226 CNRS Universit\'e Rennes 1 Bat 10C Campus de Beaulieu 35042 RENNES France ; _publ_contact_author_phone '33 2 23 23 52 43' _publ_contact_author_email marc.fourmigue@univ-rennes1.fr _publ_requested_journal 'New J. Chem.' _publ_section_title ; Perylene Salts of Unsymmetrical Nickel and Gold Dithiolene Complexes with 3:2 Stoichiometry: Conformational Polymorphism and Strong Antiferromagnetic Interactions. ; data_oj160b _database_code_depnum_ccdc_archive 'CCDC 616047' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Bu4N, cis-Au(tfadt)' _chemical_melting_point ? _chemical_formula_moiety 'C16 H36 N, Au F6 N2 S4' _chemical_formula_sum 'C24 H36 Au F6 N3 S4' _chemical_formula_weight 805.76 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.5030(12) _cell_length_b 12.2691(14) _cell_length_c 12.5077(14) _cell_angle_alpha 104.268(13) _cell_angle_beta 113.245(12) _cell_angle_gamma 92.870(12) _cell_volume 1550.2(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7998 _cell_measurement_theta_min 1.7 _cell_measurement_theta_max 25.8 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.726 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 796 _exptl_absorpt_coefficient_mu 5.069 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; a grid of 8 x 8 x 12 = 768 sampling points was used ; _exptl_absorpt_correction_T_min 0.2872 _exptl_absorpt_correction_T_max 0.5580 _exptl_absorpt_correction_T_ave 0.4682 _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS' _diffrn_measurement_method 'Oscillation, phi incr. 1.8 deg' _diffrn_detector_area_resol_mean 6.66 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14990 _diffrn_reflns_av_R_equivalents 0.0323 _diffrn_reflns_av_sigmaI/netI 0.0347 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 25.97 _reflns_number_total 5543 _reflns_number_gt 4711 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'EXPOSE, Stoe-IPDS' _computing_cell_refinement 'CELL, Stoe-IPDS' _computing_data_reduction 'INTEGRATE, Stoe-IPDS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0591P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment Constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5543 _refine_ls_number_parameters 343 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0434 _refine_ls_R_factor_gt 0.0334 _refine_ls_wR_factor_ref 0.0879 _refine_ls_wR_factor_gt 0.0825 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au1 Au 0.417226(17) 0.504548(18) 0.213830(19) 0.03469(9) Uani 1 1 d . . . S1 S 0.57407(12) 0.44859(12) 0.36418(13) 0.0399(3) Uani 1 1 d . . . S2 S 0.45129(17) 0.37205(17) 0.06747(16) 0.0603(4) Uani 1 1 d . . . S3 S 0.26216(18) 0.55560(19) 0.06040(16) 0.0645(5) Uani 1 1 d . . . S4 S 0.37702(12) 0.63717(12) 0.35675(13) 0.0378(3) Uani 1 1 d . . . C1 C 0.6176(5) 0.3371(5) 0.2755(6) 0.0401(13) Uani 1 1 d . . . C2 C 0.5655(6) 0.3058(5) 0.1550(6) 0.0483(15) Uani 1 1 d . . . C3 C 0.7177(6) 0.2826(5) 0.3463(7) 0.0508(16) Uani 1 1 d . . . C4 C 0.6051(7) 0.2089(7) 0.0865(7) 0.0636(19) Uani 1 1 d . . . C5 C 0.2057(6) 0.6593(6) 0.1398(6) 0.0494(15) Uani 1 1 d . . . C6 C 0.2544(5) 0.6948(5) 0.2615(6) 0.0393(13) Uani 1 1 d . . . C7 C 0.0993(7) 0.7122(8) 0.0659(7) 0.066(2) Uani 1 1 d . . . C8 C 0.2085(5) 0.7847(5) 0.3243(6) 0.0439(14) Uani 1 1 d . . . C1A C 0.8324(4) 0.8370(4) 0.5030(5) 0.0287(10) Uani 1 1 d . . . H1A1 H 0.9230 0.8319 0.5313 0.034 Uiso 1 1 calc R . . H1A2 H 0.8256 0.9152 0.5371 0.034 Uiso 1 1 calc R . . C2A C 0.7723(5) 0.7606(4) 0.5526(5) 0.0336(11) Uani 1 1 d . . . H2A1 H 0.7752 0.6817 0.5167 0.040 Uiso 1 1 calc R . . H2A2 H 0.6829 0.7688 0.5298 0.040 Uiso 1 1 calc R . . C3A C 0.8414(4) 0.7898(4) 0.6902(5) 0.0328(11) Uani 1 1 d . . . H3A1 H 0.8428 0.8698 0.7261 0.039 Uiso 1 1 calc R . . H3A2 H 0.9294 0.7771 0.7129 0.039 Uiso 1 1 calc R . . C4A C 0.7754(5) 0.7172(5) 0.7399(5) 0.0401(13) Uani 1 1 d . . . H4A1 H 0.8205 0.7377 0.8268 0.060 Uiso 1 1 calc R . . H4A2 H 0.7756 0.6381 0.7059 0.060 Uiso 1 1 calc R . . H4A3 H 0.6885 0.7303 0.7182 0.060 Uiso 1 1 calc R . . C5A C 0.7777(4) 0.6876(4) 0.3058(5) 0.0298(10) Uani 1 1 d . . . H5A1 H 0.7201 0.6384 0.3199 0.036 Uiso 1 1 calc R . . H5A2 H 0.7445 0.6757 0.2187 0.036 Uiso 1 1 calc R . . C6A C 0.9077(5) 0.6508(5) 0.3482(6) 0.0408(13) Uani 1 1 d . . . H6A1 H 0.9634 0.6931 0.3256 0.049 Uiso 1 1 calc R . . H6A2 H 0.9456 0.6686 0.4361 0.049 Uiso 1 1 calc R . . C7A C 0.8987(6) 0.5269(5) 0.2943(7) 0.0531(16) Uani 1 1 d . . . H7A1 H 0.8607 0.5100 0.2065 0.064 Uiso 1 1 calc R . . H7A2 H 0.8412 0.4855 0.3158 0.064 Uiso 1 1 calc R . . C8A C 1.0250(7) 0.4834(6) 0.3338(8) 0.066(2) Uani 1 1 d . . . H8A1 H 1.0108 0.4030 0.2947 0.100 Uiso 1 1 calc R . . H8A2 H 1.0622 0.4971 0.4204 0.100 Uiso 1 1 calc R . . H8A3 H 1.0823 0.5224 0.3114 0.100 Uiso 1 1 calc R . . C9A C 0.8535(4) 0.8922(4) 0.3365(5) 0.0303(11) Uani 1 1 d . . . H9A1 H 0.9420 0.8802 0.3693 0.036 Uiso 1 1 calc R . . H9A2 H 0.8513 0.9695 0.3779 0.036 Uiso 1 1 calc R . . C10A C 0.8098(5) 0.8812(5) 0.2012(5) 0.0360(12) Uani 1 1 d . . . H10A H 0.8208 0.8072 0.1598 0.043 Uiso 1 1 calc R . . H10B H 0.7194 0.8870 0.1654 0.043 Uiso 1 1 calc R . . C11A C 0.8872(5) 0.9743(5) 0.1850(6) 0.0394(12) Uani 1 1 d . . . H11A H 0.8765 1.0479 0.2276 0.047 Uiso 1 1 calc R . . H11B H 0.9773 0.9681 0.2215 0.047 Uiso 1 1 calc R . . C12A C 0.8483(7) 0.9686(6) 0.0533(7) 0.0583(17) Uani 1 1 d . . . H12A H 0.8998 1.0295 0.0482 0.087 Uiso 1 1 calc R . . H12B H 0.7595 0.9760 0.0169 0.087 Uiso 1 1 calc R . . H12C H 0.8609 0.8968 0.0109 0.087 Uiso 1 1 calc R . . C13A C 0.6349(4) 0.8254(4) 0.3161(5) 0.0329(11) Uani 1 1 d . . . H13A H 0.5977 0.7947 0.2283 0.039 Uiso 1 1 calc R . . H13B H 0.5903 0.7801 0.3462 0.039 Uiso 1 1 calc R . . C14A C 0.6095(5) 0.9457(5) 0.3472(6) 0.0423(14) Uani 1 1 d . . . H14A H 0.6572 0.9818 0.4338 0.051 Uiso 1 1 calc R . . H14B H 0.6391 0.9887 0.3046 0.051 Uiso 1 1 calc R . . C15A C 0.4691(5) 0.9475(6) 0.3125(7) 0.0540(17) Uani 1 1 d . . . H15A H 0.4214 0.9016 0.2287 0.065 Uiso 1 1 calc R . . H15B H 0.4431 0.9125 0.3628 0.065 Uiso 1 1 calc R . . C16A C 0.4338(7) 1.0640(7) 0.3253(9) 0.077(2) Uani 1 1 d . . . H16A H 0.3430 1.0584 0.3015 0.116 Uiso 1 1 calc R . . H16B H 0.4570 1.0989 0.2741 0.116 Uiso 1 1 calc R . . H16C H 0.4786 1.1097 0.4084 0.116 Uiso 1 1 calc R . . N1 N 0.7975(7) 0.2408(7) 0.4020(7) 0.089(2) Uani 1 1 d . . . N2 N 0.1746(5) 0.8576(5) 0.3732(6) 0.0570(15) Uani 1 1 d . . . N1A N 0.7745(3) 0.8103(3) 0.3654(4) 0.0264(8) Uani 1 1 d . . . F1 F 0.7356(5) 0.2289(5) 0.1163(6) 0.1033(18) Uani 1 1 d . . . F2 F 0.5499(6) 0.1815(6) -0.0268(5) 0.119(2) Uani 1 1 d . . . F3 F 0.5966(6) 0.1104(5) 0.1173(6) 0.1050(18) Uani 1 1 d . . . F4 F 0.1304(5) 0.8224(5) 0.0875(6) 0.1007(18) Uani 1 1 d . . . F5 F -0.0044(4) 0.7006(5) 0.0879(5) 0.0858(15) Uani 1 1 d . . . F6 F 0.0632(7) 0.6669(8) -0.0518(5) 0.159(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Au1 0.03054(11) 0.03587(13) 0.03282(13) 0.00902(9) 0.00937(8) 0.00215(7) S1 0.0338(6) 0.0375(7) 0.0386(8) 0.0086(7) 0.0069(5) 0.0047(5) S2 0.0650(10) 0.0688(11) 0.0368(9) 0.0067(9) 0.0146(7) 0.0255(9) S3 0.0689(11) 0.0842(13) 0.0352(9) 0.0190(9) 0.0128(8) 0.0373(10) S4 0.0344(6) 0.0403(7) 0.0365(8) 0.0126(7) 0.0119(5) 0.0069(5) C1 0.029(2) 0.031(3) 0.049(4) 0.002(3) 0.011(2) 0.001(2) C2 0.044(3) 0.040(3) 0.053(4) 0.004(3) 0.019(3) 0.003(2) C3 0.043(3) 0.041(3) 0.067(5) 0.024(3) 0.015(3) 0.016(3) C4 0.072(5) 0.059(5) 0.059(5) 0.009(4) 0.031(4) 0.008(4) C5 0.043(3) 0.058(4) 0.048(4) 0.024(3) 0.014(3) 0.021(3) C6 0.029(2) 0.039(3) 0.051(4) 0.016(3) 0.016(2) 0.007(2) C7 0.059(4) 0.083(6) 0.057(5) 0.025(5) 0.020(3) 0.028(4) C8 0.029(3) 0.044(3) 0.058(4) 0.016(3) 0.017(3) 0.005(2) C1A 0.026(2) 0.024(2) 0.032(3) 0.005(2) 0.0103(19) 0.0054(18) C2A 0.033(2) 0.027(3) 0.037(3) 0.005(2) 0.015(2) -0.0002(19) C3A 0.027(2) 0.031(3) 0.039(3) 0.009(2) 0.013(2) 0.0068(19) C4A 0.042(3) 0.041(3) 0.043(3) 0.017(3) 0.020(2) 0.009(2) C5A 0.030(2) 0.026(2) 0.028(3) 0.002(2) 0.011(2) 0.0019(19) C6A 0.037(3) 0.029(3) 0.055(4) 0.005(3) 0.021(3) 0.008(2) C7A 0.063(4) 0.034(3) 0.051(4) 0.002(3) 0.018(3) 0.016(3) C8A 0.068(4) 0.041(4) 0.093(6) 0.011(4) 0.039(4) 0.026(3) C9A 0.024(2) 0.026(2) 0.040(3) 0.009(2) 0.013(2) -0.0019(18) C10A 0.033(2) 0.034(3) 0.039(3) 0.008(3) 0.015(2) 0.001(2) C11A 0.039(3) 0.038(3) 0.046(3) 0.018(3) 0.020(2) 0.009(2) C12A 0.076(4) 0.058(4) 0.057(4) 0.026(4) 0.038(4) 0.019(3) C13A 0.020(2) 0.038(3) 0.039(3) 0.015(3) 0.009(2) 0.0046(19) C14A 0.031(3) 0.039(3) 0.059(4) 0.017(3) 0.018(2) 0.014(2) C15A 0.032(3) 0.065(4) 0.067(5) 0.024(4) 0.020(3) 0.021(3) C16A 0.058(4) 0.079(5) 0.113(7) 0.038(5) 0.045(5) 0.044(4) N1 0.072(4) 0.098(6) 0.074(5) 0.031(5) 0.006(4) 0.011(4) N2 0.039(3) 0.055(3) 0.068(4) 0.006(3) 0.019(3) 0.011(2) N1A 0.0216(18) 0.025(2) 0.032(2) 0.0074(19) 0.0108(16) 0.0024(15) F1 0.085(3) 0.108(4) 0.125(5) 0.028(4) 0.053(3) 0.028(3) F2 0.124(5) 0.151(6) 0.055(3) 0.007(4) 0.019(3) 0.062(4) F3 0.124(4) 0.065(3) 0.125(5) 0.015(3) 0.059(4) 0.019(3) F4 0.088(3) 0.112(4) 0.132(5) 0.088(4) 0.042(3) 0.045(3) F5 0.042(2) 0.110(4) 0.094(4) 0.037(3) 0.013(2) 0.021(2) F6 0.161(6) 0.249(9) 0.054(3) 0.046(5) 0.018(3) 0.152(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au1 S3 2.2933(16) . ? Au1 S2 2.3045(19) . ? Au1 S1 2.3120(14) . ? Au1 S4 2.3132(15) . ? S1 C1 1.764(6) . ? S2 C2 1.730(7) . ? S3 C5 1.730(7) . ? S4 C6 1.760(5) . ? C1 C2 1.326(9) . ? C1 C3 1.457(8) . ? C2 C4 1.489(10) . ? C3 N1 1.144(9) . ? C4 F2 1.248(9) . ? C4 F3 1.366(9) . ? C4 F1 1.389(9) . ? C5 C6 1.340(9) . ? C5 C7 1.502(9) . ? C6 C8 1.439(9) . ? C7 F4 1.313(10) . ? C7 F6 1.318(10) . ? C7 F5 1.334(9) . ? C8 N2 1.132(8) . ? C1A C2A 1.517(7) . ? C1A N1A 1.520(6) . ? C2A C3A 1.520(7) . ? C3A C4A 1.527(7) . ? C5A C6A 1.510(7) . ? C5A N1A 1.515(6) . ? C6A C7A 1.483(8) . ? C7A C8A 1.511(9) . ? C9A N1A 1.521(6) . ? C9A C10A 1.530(7) . ? C10A C11A 1.514(7) . ? C11A C12A 1.509(9) . ? C13A C14A 1.505(8) . ? C13A N1A 1.515(5) . ? C14A C15A 1.501(7) . ? C15A C16A 1.494(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S3 Au1 S2 88.26(7) . . ? S3 Au1 S1 178.28(6) . . ? S2 Au1 S1 90.03(6) . . ? S3 Au1 S4 90.27(6) . . ? S2 Au1 S4 178.35(5) . . ? S1 Au1 S4 91.44(5) . . ? C1 S1 Au1 100.8(2) . . ? C2 S2 Au1 101.7(2) . . ? C5 S3 Au1 102.2(2) . . ? C6 S4 Au1 100.6(2) . . ? C2 C1 C3 122.4(6) . . ? C2 C1 S1 123.4(5) . . ? C3 C1 S1 114.1(5) . . ? C1 C2 C4 120.3(6) . . ? C1 C2 S2 124.0(5) . . ? C4 C2 S2 115.8(5) . . ? N1 C3 C1 179.1(7) . . ? F2 C4 F3 105.9(7) . . ? F2 C4 F1 106.2(7) . . ? F3 C4 F1 100.1(6) . . ? F2 C4 C2 117.1(7) . . ? F3 C4 C2 114.4(7) . . ? F1 C4 C2 111.5(6) . . ? C6 C5 C7 120.0(6) . . ? C6 C5 S3 123.1(4) . . ? C7 C5 S3 116.9(5) . . ? C5 C6 C8 121.5(5) . . ? C5 C6 S4 123.8(5) . . ? C8 C6 S4 114.8(5) . . ? F4 C7 F6 106.1(8) . . ? F4 C7 F5 105.1(7) . . ? F6 C7 F5 107.5(7) . . ? F4 C7 C5 113.5(6) . . ? F6 C7 C5 111.8(6) . . ? F5 C7 C5 112.4(6) . . ? N2 C8 C6 178.0(6) . . ? C2A C1A N1A 115.6(4) . . ? C1A C2A C3A 111.6(4) . . ? C2A C3A C4A 111.2(4) . . ? C6A C5A N1A 115.9(4) . . ? C7A C6A C5A 111.7(5) . . ? C6A C7A C8A 114.8(5) . . ? N1A C9A C10A 115.2(4) . . ? C11A C10A C9A 110.2(4) . . ? C12A C11A C10A 112.9(5) . . ? C14A C13A N1A 116.2(4) . . ? C15A C14A C13A 111.0(5) . . ? C16A C15A C14A 114.2(6) . . ? C5A N1A C13A 106.7(3) . . ? C5A N1A C1A 111.2(4) . . ? C13A N1A C1A 111.0(4) . . ? C5A N1A C9A 110.8(4) . . ? C13A N1A C9A 110.7(4) . . ? C1A N1A C9A 106.5(3) . . ? _diffrn_measured_fraction_theta_max 0.912 _diffrn_reflns_theta_full 25.97 _diffrn_measured_fraction_theta_full 0.912 _refine_diff_density_max 1.604 _refine_diff_density_min -1.237 _refine_diff_density_rms 0.128 # Attachment 'B608420F_PerAu_corr.cif' data_ojec162 _database_code_depnum_ccdc_archive 'CCDC 616048' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '(Perylene)3, [Au(tfadt)2]2' _chemical_melting_point ? _chemical_formula_moiety '3(C20 H12), 2(C8 F6 N2 Au S4)' _chemical_formula_sum 'C76 H36 Au2 F12 N4 S8' _chemical_formula_weight 1883.50 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.8670(13) _cell_length_b 12.7568(16) _cell_length_c 13.2210(15) _cell_angle_alpha 111.176(13) _cell_angle_beta 103.135(14) _cell_angle_gamma 96.571(15) _cell_volume 1624.9(3) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 2.1 _cell_measurement_theta_max 25.8 _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.42 _exptl_crystal_size_min 0.038 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.925 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 914 _exptl_absorpt_coefficient_mu 4.853 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; a grid of 14 x 8 x 8 = 896 sampling points was used ; _exptl_absorpt_correction_T_min 0.1486 _exptl_absorpt_correction_T_max 0.8153 _exptl_absorpt_correction_T_ave 0.6558 _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS' _diffrn_measurement_method 'Oscillation, phi incr. 1.8 deg' _diffrn_detector_area_resol_mean 6.66 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15849 _diffrn_reflns_av_R_equivalents 0.0394 _diffrn_reflns_av_sigmaI/netI 0.0467 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 25.94 _reflns_number_total 5865 _reflns_number_gt 4750 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'EXPOSE, Stoe-IPDS' _computing_cell_refinement 'CELL, Stoe-IPDS' _computing_data_reduction 'INTEGRATE, Stoe-IPDS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0232P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment Constr. _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5865 _refine_ls_number_parameters 487 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0399 _refine_ls_R_factor_gt 0.0258 _refine_ls_wR_factor_ref 0.0499 _refine_ls_wR_factor_gt 0.0473 _refine_ls_goodness_of_fit_ref 0.938 _refine_ls_restrained_S_all 0.938 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au Au 0.094203(18) -0.038430(17) -0.116927(13) 0.03715(6) Uani 1 1 d . . . S1 S 0.24502(12) 0.08682(10) 0.04974(8) 0.0520(3) Uani 1 1 d . . . S2 S 0.05327(12) 0.11291(10) -0.16546(8) 0.0492(3) Uani 1 1 d . . . S3 S -0.05715(12) -0.16312(10) -0.28366(8) 0.0520(3) Uani 1 1 d . . . S4 S 0.13813(12) -0.19073(10) -0.07076(9) 0.0493(3) Uani 1 1 d . . . C1 C 0.2320(4) 0.2192(4) 0.0409(3) 0.0473(11) Uani 1 1 d . . . C2 C 0.1535(4) 0.2293(4) -0.0476(3) 0.0439(10) Uani 1 1 d . . . C3 C 0.3141(5) 0.3146(5) 0.1382(4) 0.0647(14) Uani 1 1 d . . . C4 C 0.1445(5) 0.3442(4) -0.0540(4) 0.0563(12) Uani 1 1 d . . . C5 C -0.0375(5) -0.2962(4) -0.2794(3) 0.0498(11) Uani 1 1 d . . . C6 C 0.0441(4) -0.3070(4) -0.1928(3) 0.0482(11) Uani 1 1 d . . . C7 C -0.1204(6) -0.3923(5) -0.3785(4) 0.0741(16) Uani 1 1 d . . . C8 C 0.0651(6) -0.4221(4) -0.1969(4) 0.0638(14) Uani 1 1 d . . . C1A C 0.2263(4) -0.1932(4) -0.3975(3) 0.0522(12) Uani 1 1 d . . . C2A C 0.1319(5) -0.2466(5) -0.5047(4) 0.0711(16) Uani 1 1 d . . . H2A H 0.0998 -0.3257 -0.5350 0.085 Uiso 1 1 calc R . . C3A C 0.0879(5) -0.1852(6) -0.5632(4) 0.0724(17) Uani 1 1 d . . . H3A H 0.0274 -0.2222 -0.6342 0.087 Uiso 1 1 calc R . . C4A C 0.1321(4) -0.0671(5) -0.5186(3) 0.0593(14) Uani 1 1 d . . . H4A H 0.0993 -0.0263 -0.5604 0.071 Uiso 1 1 calc R . . C5A C 0.2239(4) -0.0068(4) -0.4134(3) 0.0390(10) Uani 1 1 d . . . C6A C 0.2722(4) 0.1166(4) -0.3656(3) 0.0407(10) Uani 1 1 d . . . C7A C 0.2301(5) 0.1858(5) -0.4213(4) 0.0588(13) Uani 1 1 d . . . H7A H 0.1681 0.1515 -0.4917 0.071 Uiso 1 1 calc R . . C8A C 0.2769(6) 0.3030(6) -0.3760(5) 0.0768(17) Uani 1 1 d . . . H8A H 0.2453 0.3462 -0.4156 0.092 Uiso 1 1 calc R . . C9A C 0.3692(6) 0.3567(5) -0.2735(5) 0.0707(15) Uani 1 1 d . . . H9A H 0.4007 0.4358 -0.2443 0.085 Uiso 1 1 calc R . . C10A C 0.4164(5) 0.2931(4) -0.2121(4) 0.0537(12) Uani 1 1 d . . . C11A C 0.5112(5) 0.3452(5) -0.1052(4) 0.0716(15) Uani 1 1 d . . . H11A H 0.5444 0.4242 -0.0746 0.086 Uiso 1 1 calc R . . C12A C 0.5549(5) 0.2821(6) -0.0462(4) 0.0723(16) Uani 1 1 d . . . H12A H 0.6163 0.3185 0.0243 0.087 Uiso 1 1 calc R . . C13A C 0.5087(4) 0.1646(5) -0.0903(3) 0.0572(13) Uani 1 1 d . . . H13A H 0.5395 0.1229 -0.0487 0.069 Uiso 1 1 calc R . . C14A C 0.4161(4) 0.1067(4) -0.1965(3) 0.0423(11) Uani 1 1 d . . . C15A C 0.3694(4) -0.0168(4) -0.2432(3) 0.0408(10) Uani 1 1 d . . . C16A C 0.4137(5) -0.0871(5) -0.1891(3) 0.0559(12) Uani 1 1 d . . . H16A H 0.4762 -0.0533 -0.1189 0.067 Uiso 1 1 calc R . . C17A C 0.3686(6) -0.2040(5) -0.2355(4) 0.0672(14) Uani 1 1 d . . . H17A H 0.4012 -0.2475 -0.1968 0.081 Uiso 1 1 calc R . . C18A C 0.2773(6) -0.2568(5) -0.3370(4) 0.0690(15) Uani 1 1 d . . . H18A H 0.2478 -0.3363 -0.3672 0.083 Uiso 1 1 calc R . . C19A C 0.2734(4) -0.0712(4) -0.3512(3) 0.0392(10) Uani 1 1 d . . . C20A C 0.3682(4) 0.1717(4) -0.2574(3) 0.0397(10) Uani 1 1 d . . . C1B C 0.5953(5) 0.2428(4) 0.5963(4) 0.0556(12) Uani 1 1 d . . . C2B C 0.5483(6) 0.3079(5) 0.5368(5) 0.0721(16) Uani 1 1 d . . . H2B H 0.5782 0.3874 0.5689 0.087 Uiso 1 1 calc R . . C3B C 0.4596(6) 0.2571(5) 0.4328(5) 0.0753(17) Uani 1 1 d . . . H3B H 0.4309 0.3016 0.3938 0.090 Uiso 1 1 calc R . . C4B C 0.4119(5) 0.1393(5) 0.3851(4) 0.0598(14) Uani 1 1 d . . . H4B H 0.3503 0.1060 0.3144 0.072 Uiso 1 1 calc R . . C5B C 0.4537(4) 0.0684(4) 0.4401(3) 0.0418(10) Uani 1 1 d . . . C6B C 0.4057(4) -0.0541(4) 0.3919(3) 0.0424(11) Uani 1 1 d . . . C7B C 0.3137(4) -0.1132(5) 0.2853(3) 0.0585(13) Uani 1 1 d . . . H7B H 0.2820 -0.0712 0.2445 0.070 Uiso 1 1 calc R . . C8B C 0.2685(5) -0.2308(6) 0.2388(4) 0.0742(17) Uani 1 1 d . . . H8B H 0.2081 -0.2666 0.1676 0.089 Uiso 1 1 calc R . . C9B C 0.6881(5) 0.2944(5) 0.7035(4) 0.0725(16) Uani 1 1 d . . . H9B H 0.7203 0.3736 0.7352 0.087 Uiso 1 1 calc R . . C10B C 0.5477(4) 0.1217(4) 0.5480(3) 0.0416(10) Uani 1 1 d . . . N1 N 0.3824(6) 0.3871(5) 0.2185(4) 0.1001(18) Uani 1 1 d . . . N2 N -0.1881(7) -0.4633(4) -0.4579(4) 0.119(2) Uani 1 1 d . . . F1 F 0.2326(12) 0.4313(8) 0.0146(11) 0.094(4) Uani 0.50 1 d P . . F2 F 0.1424(11) 0.3373(8) -0.1584(7) 0.075(3) Uani 0.50 1 d P . . F3 F 0.0356(9) 0.3707(7) -0.0444(12) 0.072(2) Uani 0.50 1 d P . . F'1 F 0.2543(12) 0.3977(11) -0.0468(15) 0.119(6) Uani 0.50 1 d P . . F'2 F 0.056(2) 0.3416(9) -0.1358(16) 0.193(9) Uani 0.50 1 d P . . F'3 F 0.125(2) 0.4166(10) 0.0396(12) 0.134(4) Uani 0.50 1 d P . . F4 F 0.1279(3) -0.4192(3) -0.0978(3) 0.0959(11) Uani 1 1 d . . . F5 F -0.0437(4) -0.4991(3) -0.2298(3) 0.1147(14) Uani 1 1 d . . . F6 F 0.1287(6) -0.4668(4) -0.2662(4) 0.172(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Au 0.03758(9) 0.03657(9) 0.03722(8) 0.01462(6) 0.01010(5) 0.00973(7) S1 0.0556(8) 0.0464(7) 0.0447(5) 0.0192(5) -0.0021(5) 0.0069(6) S2 0.0556(8) 0.0403(7) 0.0452(5) 0.0179(5) 0.0008(5) 0.0108(6) S3 0.0576(8) 0.0435(7) 0.0433(5) 0.0134(5) -0.0008(5) 0.0117(6) S4 0.0547(8) 0.0439(7) 0.0496(6) 0.0239(5) 0.0070(5) 0.0109(6) C1 0.050(3) 0.040(3) 0.045(2) 0.0121(19) 0.010(2) 0.007(2) C2 0.043(3) 0.041(3) 0.049(2) 0.018(2) 0.016(2) 0.011(2) C3 0.071(4) 0.049(3) 0.058(3) 0.019(2) -0.002(3) 0.008(3) C4 0.049(3) 0.047(3) 0.070(3) 0.023(3) 0.012(3) 0.013(3) C5 0.056(3) 0.039(3) 0.052(2) 0.016(2) 0.013(2) 0.010(2) C6 0.051(3) 0.039(3) 0.054(2) 0.019(2) 0.015(2) 0.005(2) C7 0.096(5) 0.044(3) 0.062(3) 0.017(3) -0.006(3) 0.009(3) C8 0.084(4) 0.042(3) 0.071(3) 0.028(2) 0.024(3) 0.009(3) C1A 0.045(3) 0.057(3) 0.053(2) 0.015(2) 0.028(2) 0.004(2) C2A 0.058(4) 0.070(4) 0.055(3) -0.005(3) 0.023(3) -0.013(3) C3A 0.039(3) 0.092(5) 0.045(2) -0.011(3) 0.007(2) 0.000(3) C4A 0.037(3) 0.092(4) 0.038(2) 0.015(2) 0.0068(19) 0.021(3) C5A 0.025(2) 0.053(3) 0.0335(18) 0.0098(18) 0.0112(16) 0.007(2) C6A 0.031(2) 0.062(3) 0.0373(19) 0.024(2) 0.0159(17) 0.015(2) C7A 0.053(3) 0.081(4) 0.059(3) 0.040(3) 0.021(2) 0.028(3) C8A 0.081(4) 0.090(5) 0.102(4) 0.066(4) 0.047(4) 0.044(4) C9A 0.073(4) 0.050(3) 0.105(4) 0.032(3) 0.049(3) 0.022(3) C10A 0.049(3) 0.052(3) 0.060(3) 0.014(2) 0.030(2) 0.010(3) C11A 0.056(3) 0.054(3) 0.077(3) -0.005(3) 0.028(3) -0.007(3) C12A 0.053(3) 0.086(5) 0.050(3) 0.004(3) 0.008(2) 0.001(3) C13A 0.047(3) 0.073(4) 0.035(2) 0.012(2) 0.0032(19) 0.000(3) C14A 0.035(2) 0.061(3) 0.0319(18) 0.0175(19) 0.0136(17) 0.009(2) C15A 0.036(2) 0.053(3) 0.0346(19) 0.0166(18) 0.0148(17) 0.008(2) C16A 0.057(3) 0.078(4) 0.046(2) 0.034(2) 0.022(2) 0.022(3) C17A 0.088(4) 0.068(4) 0.072(3) 0.043(3) 0.042(3) 0.028(3) C18A 0.086(4) 0.054(3) 0.081(3) 0.027(3) 0.054(3) 0.011(3) C19A 0.032(2) 0.052(3) 0.0357(19) 0.0150(18) 0.0185(17) 0.008(2) C20A 0.031(2) 0.046(3) 0.0398(19) 0.0126(18) 0.0148(17) 0.006(2) C1B 0.050(3) 0.056(3) 0.060(3) 0.015(2) 0.029(2) 0.006(3) C2B 0.077(4) 0.063(4) 0.097(4) 0.037(3) 0.053(3) 0.020(3) C3B 0.099(5) 0.076(4) 0.098(4) 0.061(4) 0.059(4) 0.044(4) C4B 0.056(3) 0.087(4) 0.054(2) 0.038(3) 0.025(2) 0.031(3) C5B 0.037(2) 0.060(3) 0.0359(19) 0.021(2) 0.0202(18) 0.017(2) C6B 0.028(2) 0.064(3) 0.0336(19) 0.015(2) 0.0134(17) 0.013(2) C7B 0.044(3) 0.080(4) 0.041(2) 0.015(2) 0.010(2) 0.010(3) C8B 0.045(3) 0.093(5) 0.053(3) 0.002(3) 0.009(2) 0.000(3) C9B 0.057(4) 0.063(4) 0.075(3) 0.001(3) 0.032(3) -0.008(3) C10B 0.031(2) 0.057(3) 0.042(2) 0.019(2) 0.0209(18) 0.010(2) N1 0.109(4) 0.065(3) 0.085(3) 0.020(3) -0.021(3) -0.002(3) N2 0.171(6) 0.051(3) 0.077(3) 0.007(3) -0.031(3) 0.005(4) F1 0.081(8) 0.035(5) 0.119(7) 0.026(5) -0.043(6) -0.009(5) F2 0.125(9) 0.062(5) 0.071(5) 0.045(4) 0.048(7) 0.046(7) F3 0.051(4) 0.046(5) 0.123(6) 0.034(5) 0.028(5) 0.019(4) F'1 0.095(8) 0.071(8) 0.234(17) 0.078(10) 0.094(12) 0.027(7) F'2 0.205(17) 0.054(7) 0.200(16) 0.044(10) -0.141(12) -0.002(10) F'3 0.219(14) 0.074(7) 0.160(10) 0.049(7) 0.127(11) 0.077(9) F4 0.107(3) 0.054(2) 0.110(2) 0.0444(18) -0.014(2) 0.009(2) F5 0.114(3) 0.061(2) 0.137(3) 0.056(2) -0.030(2) -0.024(2) F6 0.304(7) 0.106(3) 0.242(5) 0.114(4) 0.211(5) 0.140(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au S2 2.3019(12) . ? Au S1 2.3044(13) . ? Au S4 2.3047(12) . ? Au S3 2.3054(13) . ? S1 C1 1.753(5) . ? S2 C2 1.734(4) . ? S3 C5 1.754(5) . ? S4 C6 1.738(4) . ? C1 C2 1.341(6) . ? C1 C3 1.425(7) . ? C2 C4 1.511(6) . ? C3 N1 1.143(6) . ? C4 F'2 1.258(10) . ? C4 F1 1.267(10) . ? C4 F'1 1.270(12) . ? C4 F3 1.288(8) . ? C4 F'3 1.330(9) . ? C4 F2 1.346(8) . ? C5 C6 1.340(6) . ? C5 C7 1.443(7) . ? C6 C8 1.495(6) . ? C7 N2 1.129(6) . ? C8 F6 1.282(6) . ? C8 F4 1.318(5) . ? C8 F5 1.321(6) . ? C1A C18A 1.405(7) . ? C1A C2A 1.417(7) . ? C1A C19A 1.431(6) . ? C2A C3A 1.340(8) . ? C3A C4A 1.383(8) . ? C4A C5A 1.393(6) . ? C5A C19A 1.424(6) . ? C5A C6A 1.447(6) . ? C6A C7A 1.393(6) . ? C6A C20A 1.433(5) . ? C7A C8A 1.376(8) . ? C8A C9A 1.366(8) . ? C9A C10A 1.401(7) . ? C10A C11A 1.416(7) . ? C10A C20A 1.426(6) . ? C11A C12A 1.362(8) . ? C12A C13A 1.379(7) . ? C13A C14A 1.403(5) . ? C14A C20A 1.413(6) . ? C14A C15A 1.447(6) . ? C15A C16A 1.398(6) . ? C15A C19A 1.431(5) . ? C16A C17A 1.369(7) . ? C17A C18A 1.352(7) . ? C1B C2B 1.399(7) . ? C1B C9B 1.408(7) . ? C1B C10B 1.421(6) . ? C2B C3B 1.360(8) . ? C3B C4B 1.384(7) . ? C4B C5B 1.404(6) . ? C5B C10B 1.421(6) . ? C5B C6B 1.437(6) . ? C6B C7B 1.404(6) . ? C6B C10B 1.429(6) 2_656 ? C7B C8B 1.377(8) . ? C8B C9B 1.354(8) 2_656 ? C9B C8B 1.354(8) 2_656 ? C10B C6B 1.429(6) 2_656 ? F1 F'1 0.870(12) . ? F1 F'3 1.299(15) . ? F2 F'2 1.05(3) . ? F2 F'1 1.549(17) . ? F3 F'3 1.193(15) . ? F3 F'2 1.21(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S2 Au S1 90.47(4) . . ? S2 Au S4 178.77(5) . . ? S1 Au S4 89.70(4) . . ? S2 Au S3 89.31(4) . . ? S1 Au S3 179.75(5) . . ? S4 Au S3 90.52(4) . . ? C1 S1 Au 100.78(14) . . ? C2 S2 Au 101.46(14) . . ? C5 S3 Au 100.72(15) . . ? C6 S4 Au 101.12(15) . . ? C2 C1 C3 123.8(4) . . ? C2 C1 S1 123.7(3) . . ? C3 C1 S1 112.6(3) . . ? C1 C2 C4 122.8(4) . . ? C1 C2 S2 123.5(4) . . ? C4 C2 S2 113.6(3) . . ? N1 C3 C1 176.3(6) . . ? F'2 C4 F1 125.8(8) . . ? F'2 C4 F'1 112.4(12) . . ? F1 C4 F'1 40.1(6) . . ? F'2 C4 F3 56.8(11) . . ? F1 C4 F3 106.9(7) . . ? F'1 C4 F3 135.9(7) . . ? F'2 C4 F'3 106.3(12) . . ? F1 C4 F'3 60.0(8) . . ? F'1 C4 F'3 99.8(9) . . ? F3 C4 F'3 54.2(7) . . ? F'2 C4 F2 47.2(12) . . ? F1 C4 F2 106.1(9) . . ? F'1 C4 F2 72.6(8) . . ? F3 C4 F2 102.9(7) . . ? F'3 C4 F2 138.7(7) . . ? F'2 C4 C2 115.7(6) . . ? F1 C4 C2 118.1(5) . . ? F'1 C4 C2 110.7(7) . . ? F3 C4 C2 111.9(5) . . ? F'3 C4 C2 110.8(5) . . ? F2 C4 C2 109.8(5) . . ? C6 C5 C7 123.9(4) . . ? C6 C5 S3 123.6(4) . . ? C7 C5 S3 112.4(3) . . ? C5 C6 C8 121.7(4) . . ? C5 C6 S4 123.6(4) . . ? C8 C6 S4 114.7(3) . . ? N2 C7 C5 176.2(6) . . ? F6 C8 F4 106.8(5) . . ? F6 C8 F5 105.4(5) . . ? F4 C8 F5 104.7(4) . . ? F6 C8 C6 112.6(4) . . ? F4 C8 C6 113.3(4) . . ? F5 C8 C6 113.3(5) . . ? C18A C1A C2A 122.0(5) . . ? C18A C1A C19A 119.2(4) . . ? C2A C1A C19A 118.7(5) . . ? C3A C2A C1A 121.3(5) . . ? C2A C3A C4A 120.3(5) . . ? C3A C4A C5A 122.6(5) . . ? C4A C5A C19A 117.7(4) . . ? C4A C5A C6A 123.4(4) . . ? C19A C5A C6A 118.8(3) . . ? C7A C6A C20A 117.5(4) . . ? C7A C6A C5A 122.6(4) . . ? C20A C6A C5A 119.9(4) . . ? C8A C7A C6A 122.4(5) . . ? C9A C8A C7A 120.7(5) . . ? C8A C9A C10A 120.3(5) . . ? C9A C10A C11A 122.2(5) . . ? C9A C10A C20A 119.6(4) . . ? C11A C10A C20A 118.1(5) . . ? C12A C11A C10A 121.4(5) . . ? C11A C12A C13A 120.5(5) . . ? C12A C13A C14A 121.3(5) . . ? C13A C14A C20A 118.6(4) . . ? C13A C14A C15A 121.1(4) . . ? C20A C14A C15A 120.2(4) . . ? C16A C15A C19A 117.7(4) . . ? C16A C15A C14A 123.6(4) . . ? C19A C15A C14A 118.8(4) . . ? C17A C16A C15A 122.4(4) . . ? C18A C17A C16A 120.9(5) . . ? C17A C18A C1A 120.8(5) . . ? C5A C19A C1A 119.4(4) . . ? C5A C19A C15A 121.6(4) . . ? C1A C19A C15A 119.0(4) . . ? C14A C20A C10A 120.0(4) . . ? C14A C20A C6A 120.6(4) . . ? C10A C20A C6A 119.4(4) . . ? C2B C1B C9B 121.7(5) . . ? C2B C1B C10B 119.3(5) . . ? C9B C1B C10B 119.0(5) . . ? C3B C2B C1B 121.2(5) . . ? C2B C3B C4B 120.1(5) . . ? C3B C4B C5B 121.9(5) . . ? C4B C5B C10B 117.8(4) . . ? C4B C5B C6B 122.8(4) . . ? C10B C5B C6B 119.4(4) . . ? C7B C6B C10B 117.0(4) . 2_656 ? C7B C6B C5B 122.8(4) . . ? C10B C6B C5B 120.2(4) 2_656 . ? C8B C7B C6B 122.8(5) . . ? C9B C8B C7B 120.1(5) 2_656 . ? C8B C9B C1B 121.2(5) 2_656 . ? C1B C10B C5B 119.7(4) . . ? C1B C10B C6B 119.9(4) . 2_656 ? C5B C10B C6B 120.4(4) . 2_656 ? F'1 F1 C4 70.1(11) . . ? F'1 F1 F'3 131.8(16) . . ? C4 F1 F'3 62.4(7) . . ? F'2 F2 C4 62.0(9) . . ? F'2 F2 F'1 106.5(11) . . ? C4 F2 F'1 51.5(5) . . ? F'3 F3 F'2 119.0(11) . . ? F'3 F3 C4 64.7(6) . . ? F'2 F3 C4 60.4(8) . . ? F1 F'1 C4 69.8(11) . . ? F1 F'1 F2 116.6(15) . . ? C4 F'1 F2 56.0(7) . . ? F2 F'2 F3 131.6(12) . . ? F2 F'2 C4 70.8(10) . . ? F3 F'2 C4 62.8(8) . . ? F3 F'3 F1 110.8(9) . . ? F3 F'3 C4 61.1(7) . . ? F1 F'3 C4 57.6(5) . . ? _diffrn_measured_fraction_theta_max 0.922 _diffrn_reflns_theta_full 25.94 _diffrn_measured_fraction_theta_full 0.922 _refine_diff_density_max 0.564 _refine_diff_density_min -0.501 _refine_diff_density_rms 0.085 # Attachment 'B608420F_PerNi.cif' data_ojec111 _database_code_depnum_ccdc_archive 'CCDC 616049' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (perylene)1.5,[Ni(tfadt)2] _chemical_melting_point ? _chemical_formula_moiety '1.5(C20 H12), C8 F6 N2 Ni S4' _chemical_formula_sum 'C38 H18 F6 N2 Ni S4' _chemical_formula_weight 803.49 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.8853(14) _cell_length_b 12.6566(14) _cell_length_c 13.1882(16) _cell_angle_alpha 113.253(13) _cell_angle_beta 103.614(14) _cell_angle_gamma 94.149(14) _cell_volume 1594.4(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6536 _cell_measurement_theta_min 1.8 _cell_measurement_theta_max 25.25 _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 0.56 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.674 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 812 _exptl_absorpt_coefficient_mu 0.940 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; a grid of 8 x 8 x 8 = 512 sampling points was used ; _exptl_absorpt_correction_T_min 0.6801 _exptl_absorpt_correction_T_max 0.9650 _exptl_absorpt_correction_T_ave 0.9137 _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS' _diffrn_measurement_method 'Rotation, phi incr. 1.8 deg' _diffrn_detector_area_resol_mean 6.66 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15531 _diffrn_reflns_av_R_equivalents 0.0516 _diffrn_reflns_av_sigmaI/netI 0.0803 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 25.99 _reflns_number_total 5735 _reflns_number_gt 2597 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'EXPOSE, Stoe-IPDS' _computing_cell_refinement 'CELL, Stoe-IPDS' _computing_data_reduction 'INTEGRATE, Stoe-IPDS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0793P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0022(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5735 _refine_ls_number_parameters 515 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1187 _refine_ls_R_factor_gt 0.0460 _refine_ls_wR_factor_ref 0.1385 _refine_ls_wR_factor_gt 0.1111 _refine_ls_goodness_of_fit_ref 0.823 _refine_ls_restrained_S_all 0.823 _refine_ls_shift/su_max 0.034 _refine_ls_shift/su_mean 0.003 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni Ni 0.59763(7) 0.47401(5) 0.39947(6) 0.0522(2) Uani 1 1 d . . . S1 S 0.74380(13) 0.58598(10) 0.55468(11) 0.0624(4) Uani 1 1 d . . . S2 S 0.55593(13) 0.61705(10) 0.35788(12) 0.0654(4) Uani 1 1 d . . . S3 S 0.45089(14) 0.36344(10) 0.24459(12) 0.0657(4) Uani 1 1 d . . . S4 S 0.64302(13) 0.32896(10) 0.43700(11) 0.0600(4) Uani 1 1 d . . . C1 C 0.7428(5) 0.7234(4) 0.5547(5) 0.0601(13) Uani 1 1 d . . . C2 C 0.6612(5) 0.7351(4) 0.4680(5) 0.0580(13) Uani 1 1 d . . . C3 C 0.6524(6) 0.8502(4) 0.4585(6) 0.0692(15) Uani 1 1 d . . . C4 C 0.8340(6) 0.8166(5) 0.6514(5) 0.0771(16) Uani 1 1 d . . . C5 C 0.4630(5) 0.2248(4) 0.2367(5) 0.0615(13) Uani 1 1 d . . . C6 C 0.5469(5) 0.2104(4) 0.3192(5) 0.0591(13) Uani 1 1 d . . . C7 C 0.3756(7) 0.1306(5) 0.1354(6) 0.092(2) Uani 1 1 d . . . C8 C 0.5667(7) 0.0921(5) 0.3106(6) 0.0767(18) Uani 1 1 d . . . C1A C 0.7011(6) 0.3076(5) 0.0797(5) 0.0723(16) Uani 1 1 d . . . C2A C 0.7411(7) 0.2342(5) 0.1321(6) 0.090(2) Uani 1 1 d . . . H2A H 0.7043 0.1551 0.0957 0.108 Uiso 1 1 calc R . . C3A C 0.8327(7) 0.2766(5) 0.2351(7) 0.090(2) Uani 1 1 d . . . H3A H 0.8584 0.2264 0.2686 0.108 Uiso 1 1 calc R . . C4A C 0.8888(6) 0.3948(5) 0.2913(5) 0.0769(16) Uani 1 1 d . . . H4A H 0.9519 0.4224 0.3617 0.092 Uiso 1 1 calc R . . C5A C 0.8520(5) 0.4727(4) 0.2437(4) 0.0557(12) Uani 1 1 d . . . C6A C 0.9079(4) 0.5972(4) 0.3010(4) 0.0547(12) Uani 1 1 d . . . C7A C 0.9999(5) 0.6457(5) 0.4090(5) 0.0724(15) Uani 1 1 d . . . H7A H 1.0255 0.5982 0.4457 0.087 Uiso 1 1 calc R . . C8A C 1.0532(6) 0.7635(6) 0.4618(5) 0.0854(19) Uani 1 1 d . . . H8A H 1.1135 0.7946 0.5340 0.102 Uiso 1 1 calc R . . C9A C 1.0182(6) 0.8343(5) 0.4090(6) 0.0807(18) Uani 1 1 d . . . H9A H 1.0571 0.9128 0.4450 0.097 Uiso 1 1 calc R . . C10A C 0.9260(5) 0.7923(4) 0.3027(5) 0.0658(14) Uani 1 1 d . . . C11A C 0.8900(6) 0.8643(5) 0.2487(6) 0.0824(18) Uani 1 1 d . . . H11A H 0.9275 0.9433 0.2849 0.099 Uiso 1 1 calc R . . C12A C 0.8017(7) 0.8221(5) 0.1447(7) 0.0859(19) Uani 1 1 d . . . H12A H 0.7787 0.8723 0.1105 0.103 Uiso 1 1 calc R . . C13A C 0.7442(5) 0.7038(5) 0.0876(5) 0.0739(15) Uani 1 1 d . . . H13A H 0.6837 0.6762 0.0157 0.089 Uiso 1 1 calc R . . C14A C 0.7766(5) 0.6264(4) 0.1372(4) 0.0544(12) Uani 1 1 d . . . C15A C 0.7198(4) 0.5015(4) 0.0804(4) 0.0560(12) Uani 1 1 d . . . C16A C 0.6282(5) 0.4526(5) -0.0288(5) 0.0726(15) Uani 1 1 d . . . H16A H 0.6042 0.5000 -0.0660 0.087 Uiso 1 1 calc R . . C17A C 0.5734(6) 0.3349(6) -0.0815(6) 0.090(2) Uani 1 1 d . . . H17A H 0.5126 0.3043 -0.1534 0.108 Uiso 1 1 calc R . . C18A C 0.6079(6) 0.2640(6) -0.0292(6) 0.088(2) Uani 1 1 d . . . H18A H 0.5695 0.1853 -0.0655 0.105 Uiso 1 1 calc R . . C19A C 0.7579(5) 0.4291(4) 0.1361(5) 0.0577(13) Uani 1 1 d . . . C20A C 0.8686(5) 0.6701(4) 0.2458(4) 0.0537(12) Uani 1 1 d . . . C1B C 1.0945(4) 0.5482(4) 0.1107(4) 0.0488(11) Uani 1 1 d . . . C2B C 1.1851(5) 0.5973(5) 0.2193(4) 0.0648(14) Uani 1 1 d . . . H2B H 1.2097 0.5496 0.2562 0.078 Uiso 1 1 calc R . . C3B C 1.2389(5) 0.7148(5) 0.2731(5) 0.0734(16) Uani 1 1 d . . . H3B H 1.2988 0.7456 0.3455 0.088 Uiso 1 1 calc R . . C4B C 1.2044(5) 0.7854(5) 0.2205(5) 0.0742(17) Uani 1 1 d . . . H4B H 1.2428 0.8641 0.2571 0.089 Uiso 1 1 calc R . . C5B C 1.1119(5) 0.7429(4) 0.1116(4) 0.0600(13) Uani 1 1 d . . . C6B C 1.0552(4) 0.6203(4) 0.0551(4) 0.0484(11) Uani 1 1 d . . . C7B C 0.9628(4) 0.5761(4) -0.0545(4) 0.0486(11) Uani 1 1 d . . . C8B C 0.9289(5) 0.6538(5) -0.1035(5) 0.0680(14) Uani 1 1 d . . . H8B H 0.8678 0.6260 -0.1750 0.082 Uiso 1 1 calc R . . C9B C 0.9848(6) 0.7716(5) -0.0472(6) 0.0763(17) Uani 1 1 d . . . H9B H 0.9609 0.8215 -0.0817 0.092 Uiso 1 1 calc R . . C10B C 1.0735(6) 0.8147(5) 0.0568(6) 0.0761(17) Uani 1 1 d . . . H10B H 1.1100 0.8939 0.0928 0.091 Uiso 1 1 calc R . . F1 F 0.6434(17) 0.8394(11) 0.3521(8) 0.092(6) Uani 0.50 1 d P . . F2 F 0.556(3) 0.8911(19) 0.481(3) 0.161(13) Uani 0.50 1 d P . . F3 F 0.7531(14) 0.9287(12) 0.5186(17) 0.106(5) Uani 0.50 1 d P . . F'1 F 0.721(4) 0.871(2) 0.407(4) 0.247(15) Uani 0.50 1 d P . . F'2 F 0.5394(16) 0.8646(17) 0.426(3) 0.176(15) Uani 0.50 1 d P . . F'3 F 0.691(4) 0.9413(14) 0.5616(16) 0.182(10) Uani 0.50 1 d P . . F4 F 0.6374(13) 0.0935(12) 0.4145(11) 0.078(3) Uani 0.50 1 d P . . F'4 F 0.629(3) 0.0876(16) 0.391(2) 0.228(14) Uani 0.50 1 d P . . F5 F 0.4592(9) 0.0149(7) 0.2780(7) 0.075(3) Uani 0.50 1 d P . . F'5 F 0.444(2) 0.0220(16) 0.271(2) 0.299(15) Uani 0.50 1 d P . . F6 F 0.600(3) 0.0279(17) 0.223(3) 0.242(13) Uani 0.50 1 d P . . F'6 F 0.638(2) 0.0481(12) 0.2420(17) 0.143(7) Uani 0.50 1 d P . . N1 N 0.9077(6) 0.8868(5) 0.7280(5) 0.119(2) Uani 1 1 d . . . N2 N 0.3099(8) 0.0591(5) 0.0537(6) 0.164(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni 0.0550(4) 0.0430(3) 0.0584(4) 0.0215(2) 0.0157(3) 0.0098(2) S1 0.0681(9) 0.0509(7) 0.0627(8) 0.0248(6) 0.0088(7) 0.0073(6) S2 0.0684(9) 0.0469(7) 0.0724(9) 0.0263(6) 0.0045(7) 0.0077(6) S3 0.0714(9) 0.0484(7) 0.0681(9) 0.0241(6) 0.0050(7) 0.0104(6) S4 0.0666(9) 0.0498(7) 0.0635(8) 0.0269(6) 0.0132(7) 0.0112(6) C1 0.065(3) 0.046(3) 0.067(3) 0.020(2) 0.024(3) 0.008(2) C2 0.062(3) 0.045(2) 0.070(3) 0.024(2) 0.027(3) 0.009(2) C3 0.070(4) 0.057(3) 0.082(4) 0.031(3) 0.022(4) 0.013(3) C4 0.087(4) 0.057(3) 0.072(4) 0.022(3) 0.009(3) 0.002(3) C5 0.062(3) 0.048(3) 0.068(3) 0.018(2) 0.020(3) 0.009(2) C6 0.064(3) 0.047(3) 0.071(3) 0.025(2) 0.026(3) 0.013(2) C7 0.117(5) 0.053(3) 0.078(4) 0.020(3) -0.004(4) 0.001(3) C8 0.095(5) 0.060(4) 0.083(5) 0.039(3) 0.024(4) 0.020(4) C1A 0.075(4) 0.065(3) 0.080(4) 0.020(3) 0.048(4) 0.009(3) C2A 0.114(6) 0.059(4) 0.099(5) 0.019(4) 0.064(5) 0.002(4) C3A 0.128(6) 0.068(4) 0.115(6) 0.056(4) 0.074(5) 0.032(4) C4A 0.092(4) 0.094(4) 0.073(4) 0.049(3) 0.046(3) 0.031(3) C5A 0.059(3) 0.067(3) 0.051(3) 0.027(3) 0.028(3) 0.018(2) C6A 0.048(3) 0.065(3) 0.048(3) 0.018(2) 0.019(2) 0.006(2) C7A 0.068(4) 0.086(4) 0.058(3) 0.025(3) 0.019(3) 0.013(3) C8A 0.064(4) 0.106(5) 0.059(4) 0.009(4) 0.017(3) 0.005(4) C9A 0.064(4) 0.065(3) 0.085(4) 0.002(3) 0.029(4) 0.000(3) C10A 0.060(3) 0.059(3) 0.077(4) 0.020(3) 0.033(3) 0.010(3) C11A 0.084(5) 0.067(4) 0.107(5) 0.035(4) 0.049(4) 0.022(3) C12A 0.099(5) 0.078(4) 0.119(6) 0.060(4) 0.060(5) 0.043(4) C13A 0.070(4) 0.098(4) 0.074(4) 0.047(3) 0.033(3) 0.037(3) C14A 0.049(3) 0.066(3) 0.057(3) 0.030(3) 0.021(3) 0.019(2) C15A 0.045(3) 0.074(3) 0.049(3) 0.021(3) 0.022(2) 0.014(2) C16A 0.053(3) 0.093(4) 0.063(3) 0.022(3) 0.019(3) 0.018(3) C17A 0.053(4) 0.114(5) 0.071(4) 0.010(4) 0.018(3) 0.002(4) C18A 0.071(4) 0.075(4) 0.086(5) -0.002(4) 0.039(4) -0.010(3) C19A 0.049(3) 0.062(3) 0.064(3) 0.020(3) 0.032(3) 0.008(2) C20A 0.050(3) 0.060(3) 0.056(3) 0.023(2) 0.028(3) 0.014(2) C1B 0.041(3) 0.060(3) 0.043(3) 0.017(2) 0.016(2) 0.009(2) C2B 0.053(3) 0.081(4) 0.049(3) 0.017(3) 0.015(3) 0.012(3) C3B 0.058(3) 0.084(4) 0.055(3) 0.010(3) 0.015(3) 0.000(3) C4B 0.063(4) 0.063(3) 0.068(4) -0.001(3) 0.026(3) -0.009(3) C5B 0.060(3) 0.053(3) 0.063(3) 0.016(3) 0.028(3) 0.006(2) C6B 0.044(3) 0.051(3) 0.048(3) 0.014(2) 0.022(2) 0.006(2) C7B 0.044(3) 0.058(3) 0.048(3) 0.024(2) 0.020(2) 0.012(2) C8B 0.075(4) 0.077(4) 0.065(3) 0.035(3) 0.030(3) 0.024(3) C9B 0.099(5) 0.067(4) 0.088(4) 0.043(3) 0.049(4) 0.030(3) C10B 0.087(4) 0.058(3) 0.088(4) 0.026(3) 0.043(4) 0.012(3) F1 0.146(15) 0.058(4) 0.069(4) 0.037(4) 0.013(6) 0.008(6) F2 0.19(2) 0.104(12) 0.31(3) 0.124(15) 0.20(2) 0.101(15) F3 0.099(9) 0.053(8) 0.134(12) 0.040(8) -0.008(8) -0.032(7) F'1 0.33(3) 0.17(2) 0.48(4) 0.23(3) 0.34(3) 0.16(2) F'2 0.078(10) 0.086(9) 0.33(3) 0.113(13) -0.042(16) 0.002(7) F'3 0.27(3) 0.060(6) 0.137(13) -0.001(7) -0.008(15) 0.025(12) F4 0.089(7) 0.066(7) 0.081(5) 0.044(5) 0.006(6) 0.016(5) F'4 0.23(2) 0.069(10) 0.30(3) 0.102(14) -0.099(19) -0.033(10) F5 0.079(6) 0.041(4) 0.084(5) 0.042(4) -0.033(5) -0.019(4) F'5 0.31(3) 0.108(12) 0.44(3) 0.032(15) 0.22(2) -0.059(13) F6 0.30(3) 0.090(9) 0.27(2) -0.007(10) 0.099(19) 0.054(12) F'6 0.262(17) 0.099(8) 0.213(15) 0.120(10) 0.203(15) 0.127(10) N1 0.137(5) 0.074(3) 0.097(4) 0.022(3) -0.014(4) -0.014(3) N2 0.227(9) 0.077(4) 0.118(5) 0.023(4) -0.038(6) 0.008(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni S3 2.1367(17) . ? Ni S2 2.1379(14) . ? Ni S1 2.1401(16) . ? Ni S4 2.1430(14) . ? S1 C1 1.740(5) . ? S2 C2 1.706(5) . ? S3 C5 1.733(5) . ? S4 C6 1.711(5) . ? C1 C2 1.339(7) . ? C1 C4 1.432(7) . ? C2 C3 1.518(7) . ? C3 F'1 1.201(16) . ? C3 F2 1.245(15) . ? C3 F'2 1.254(16) . ? C3 F3 1.276(13) . ? C3 F'3 1.333(16) . ? C3 F1 1.334(14) . ? C4 N1 1.123(7) . ? C5 C6 1.327(7) . ? C5 C7 1.445(8) . ? C6 C8 1.493(7) . ? C7 N2 1.126(8) . ? C8 F'4 1.14(2) . ? C8 F6 1.28(2) . ? C8 F'6 1.312(13) . ? C8 F5 1.332(11) . ? C8 F4 1.398(17) . ? C8 F'5 1.41(2) . ? C1A C2A 1.398(9) . ? C1A C18A 1.416(9) . ? C1A C19A 1.429(7) . ? C2A C3A 1.356(9) . ? C3A C4A 1.392(8) . ? C4A C5A 1.398(7) . ? C5A C19A 1.408(7) . ? C5A C6A 1.459(7) . ? C6A C7A 1.399(7) . ? C6A C20A 1.417(7) . ? C7A C8A 1.381(8) . ? C8A C9A 1.360(9) . ? C9A C10A 1.388(8) . ? C10A C11A 1.387(8) . ? C10A C20A 1.438(7) . ? C11A C12A 1.348(9) . ? C12A C13A 1.396(8) . ? C13A C14A 1.401(7) . ? C14A C20A 1.407(7) . ? C14A C15A 1.465(7) . ? C15A C16A 1.407(7) . ? C15A C19A 1.413(7) . ? C16A C17A 1.384(8) . ? C17A C18A 1.356(9) . ? C1B C2B 1.398(6) . ? C1B C6B 1.410(6) . ? C1B C7B 1.461(6) 2_765 ? C2B C3B 1.380(7) . ? C3B C4B 1.355(8) . ? C4B C5B 1.413(7) . ? C5B C10B 1.398(7) . ? C5B C6B 1.441(6) . ? C6B C7B 1.418(6) . ? C7B C8B 1.400(7) . ? C7B C1B 1.461(6) 2_765 ? C8B C9B 1.388(7) . ? C9B C10B 1.350(8) . ? F1 F'1 0.91(5) . ? F1 F'2 1.63(3) . ? F2 F'2 0.63(4) . ? F2 F'3 1.51(3) . ? F3 F'3 0.96(3) . ? F3 F'1 1.30(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S3 Ni S2 87.40(6) . . ? S3 Ni S1 179.51(6) . . ? S2 Ni S1 92.17(6) . . ? S3 Ni S4 92.21(6) . . ? S2 Ni S4 178.07(7) . . ? S1 Ni S4 88.23(6) . . ? C1 S1 Ni 103.2(2) . . ? C2 S2 Ni 103.9(2) . . ? C5 S3 Ni 102.8(2) . . ? C6 S4 Ni 103.43(19) . . ? C2 C1 C4 125.3(5) . . ? C2 C1 S1 119.9(4) . . ? C4 C1 S1 114.8(4) . . ? C1 C2 C3 124.5(5) . . ? C1 C2 S2 120.8(4) . . ? C3 C2 S2 114.6(4) . . ? F'1 C3 F2 129.7(14) . . ? F'1 C3 F'2 112.9(18) . . ? F2 C3 F'2 29.4(17) . . ? F'1 C3 F3 63(2) . . ? F2 C3 F3 109.2(13) . . ? F'2 C3 F3 127.8(11) . . ? F'1 C3 F'3 103.9(16) . . ? F2 C3 F'3 71.7(12) . . ? F'2 C3 F'3 98.9(13) . . ? F3 C3 F'3 43.3(12) . . ? F'1 C3 F1 42(2) . . ? F2 C3 F1 104.7(15) . . ? F'2 C3 F1 78.1(16) . . ? F3 C3 F1 102.3(10) . . ? F'3 C3 F1 133.0(13) . . ? F'1 C3 C2 113.9(9) . . ? F2 C3 C2 113.9(10) . . ? F'2 C3 C2 114.0(10) . . ? F3 C3 C2 113.7(8) . . ? F'3 C3 C2 111.8(10) . . ? F1 C3 C2 112.0(7) . . ? N1 C4 C1 177.6(7) . . ? C6 C5 C7 124.7(5) . . ? C6 C5 S3 120.8(4) . . ? C7 C5 S3 114.5(4) . . ? C5 C6 C8 122.1(5) . . ? C5 C6 S4 120.5(4) . . ? C8 C6 S4 117.3(5) . . ? N2 C7 C5 176.9(8) . . ? F'4 C8 F6 109(2) . . ? F'4 C8 F'6 97.7(17) . . ? F6 C8 F'6 19(2) . . ? F'4 C8 F5 105.1(13) . . ? F6 C8 F5 91.5(15) . . ? F'6 C8 F5 109.4(11) . . ? F'4 C8 F4 5.2(17) . . ? F6 C8 F4 114.2(17) . . ? F'6 C8 F4 102.6(11) . . ? F5 C8 F4 104.4(8) . . ? F'4 C8 F'5 112.1(18) . . ? F6 C8 F'5 93.6(17) . . ? F'6 C8 F'5 112.1(15) . . ? F5 C8 F'5 8.5(12) . . ? F4 C8 F'5 110.9(14) . . ? F'4 C8 C6 117.1(11) . . ? F6 C8 C6 115.8(12) . . ? F'6 C8 C6 111.0(6) . . ? F5 C8 C6 115.1(6) . . ? F4 C8 C6 113.4(8) . . ? F'5 C8 C6 106.9(11) . . ? C2A C1A C18A 121.6(6) . . ? C2A C1A C19A 119.3(6) . . ? C18A C1A C19A 119.2(6) . . ? C3A C2A C1A 120.9(6) . . ? C2A C3A C4A 120.5(6) . . ? C3A C4A C5A 121.2(6) . . ? C4A C5A C19A 118.7(5) . . ? C4A C5A C6A 122.4(5) . . ? C19A C5A C6A 118.9(5) . . ? C7A C6A C20A 119.4(5) . . ? C7A C6A C5A 121.4(5) . . ? C20A C6A C5A 119.2(4) . . ? C8A C7A C6A 120.8(6) . . ? C9A C8A C7A 120.5(6) . . ? C8A C9A C10A 121.7(6) . . ? C11A C10A C9A 121.8(6) . . ? C11A C10A C20A 119.1(5) . . ? C9A C10A C20A 119.0(5) . . ? C12A C11A C10A 121.2(6) . . ? C11A C12A C13A 120.8(6) . . ? C12A C13A C14A 120.8(6) . . ? C13A C14A C20A 118.6(5) . . ? C13A C14A C15A 122.8(5) . . ? C20A C14A C15A 118.6(4) . . ? C16A C15A C19A 119.5(5) . . ? C16A C15A C14A 121.1(5) . . ? C19A C15A C14A 119.4(4) . . ? C17A C16A C15A 121.0(6) . . ? C18A C17A C16A 120.5(6) . . ? C17A C18A C1A 121.2(6) . . ? C5A C19A C15A 121.9(4) . . ? C5A C19A C1A 119.5(5) . . ? C15A C19A C1A 118.7(5) . . ? C14A C20A C6A 122.0(4) . . ? C14A C20A C10A 119.4(5) . . ? C6A C20A C10A 118.5(5) . . ? C2B C1B C6B 119.6(4) . . ? C2B C1B C7B 121.2(5) . 2_765 ? C6B C1B C7B 119.2(4) . 2_765 ? C3B C2B C1B 121.5(5) . . ? C4B C3B C2B 120.0(5) . . ? C3B C4B C5B 121.9(5) . . ? C10B C5B C4B 122.8(5) . . ? C10B C5B C6B 118.9(5) . . ? C4B C5B C6B 118.3(5) . . ? C1B C6B C7B 122.3(4) . . ? C1B C6B C5B 118.7(4) . . ? C7B C6B C5B 119.0(5) . . ? C8B C7B C6B 118.6(4) . . ? C8B C7B C1B 122.9(5) . 2_765 ? C6B C7B C1B 118.5(4) . 2_765 ? C9B C8B C7B 121.3(5) . . ? C10B C9B C8B 120.7(6) . . ? C9B C10B C5B 121.5(5) . . ? F'1 F1 C3 61.4(16) . . ? F'1 F1 F'2 104(2) . . ? C3 F1 F'2 48.8(9) . . ? F'2 F2 C3 76(2) . . ? F'2 F2 F'3 128(3) . . ? C3 F2 F'3 56.9(9) . . ? F'3 F3 C3 71.5(15) . . ? F'3 F3 F'1 123(2) . . ? C3 F3 F'1 55.5(12) . . ? F1 F'1 C3 77(2) . . ? F1 F'1 F3 133(3) . . ? C3 F'1 F3 61.1(14) . . ? F2 F'2 C3 74(3) . . ? F2 F'2 F1 122(3) . . ? C3 F'2 F1 53.1(11) . . ? F3 F'3 C3 65.2(14) . . ? F3 F'3 F2 110(2) . . ? C3 F'3 F2 51.5(9) . . ? _diffrn_measured_fraction_theta_max 0.916 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 0.916 _refine_diff_density_max 0.569 _refine_diff_density_min -0.518 _refine_diff_density_rms 0.066 # Attachment 'B608420F_aupph4.cif' data_aupph4 _database_code_depnum_ccdc_archive 'CCDC 616050' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'PPh4+, Au(tfadt)2-' _chemical_melting_point ? _chemical_formula_moiety 'C24 H20 P, C8 Au F6 N2 S4' _chemical_formula_sum 'C32 H20 Au F6 N2 P S4' _chemical_formula_weight 902.68 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 25.7658(12) _cell_length_b 8.0568(5) _cell_length_c 17.6766(9) _cell_angle_alpha 90.00 _cell_angle_beta 117.347(4) _cell_angle_gamma 90.00 _cell_volume 3259.4(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 125 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 27.54 _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.017 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.840 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1752 _exptl_absorpt_coefficient_mu 4.880 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6334 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details sadabs _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizontally mounted graphite crystal' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11788 _diffrn_reflns_av_R_equivalents 0.0295 _diffrn_reflns_av_sigmaI/netI 0.0384 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.38 _diffrn_reflns_theta_max 27.52 _reflns_number_total 3728 _reflns_number_gt 2700 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)' _computing_data_reduction 'EvalCCD (Duisenberg & Schreurs 1990-2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0685P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0051(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3728 _refine_ls_number_parameters 238 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0640 _refine_ls_R_factor_gt 0.0397 _refine_ls_wR_factor_ref 0.1187 _refine_ls_wR_factor_gt 0.1022 _refine_ls_goodness_of_fit_ref 1.148 _refine_ls_restrained_S_all 1.148 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au Au 0.2500 0.2500 0.0000 0.04212(16) Uani 1 2 d S . . P P 0.5000 0.0858(2) 0.2500 0.0420(5) Uani 1 2 d S . . S1 S 0.16596(7) 0.2079(2) 0.01190(11) 0.0533(4) Uani 1 1 d . . . S2 S 0.28030(6) 0.4385(2) 0.10854(10) 0.0608(4) Uani 1 1 d . . . C1 C 0.1738(2) 0.3539(7) 0.0891(3) 0.0448(12) Uani 1 1 d . . . C2 C 0.2210(2) 0.4500(7) 0.1283(3) 0.0515(13) Uani 1 1 d . . . C3 C 0.1252(3) 0.3578(7) 0.1057(4) 0.0554(14) Uani 1 1 d . . . C4 C 0.2261(3) 0.5796(10) 0.1932(5) 0.0680(18) Uani 1 1 d . . . C1A C 0.4420(2) -0.0462(7) 0.1803(3) 0.0499(13) Uani 1 1 d . . . C2A C 0.4557(4) -0.1763(12) 0.1417(6) 0.084(2) Uani 1 1 d . . . H2A H 0.4942 -0.1959 0.1534 0.100 Uiso 1 1 calc R . . C3A C 0.4113(6) -0.2765(13) 0.0855(8) 0.108(5) Uani 1 1 d . . . H3A H 0.4201 -0.3649 0.0594 0.130 Uiso 1 1 calc R . . C4A C 0.3564(6) -0.2480(10) 0.0684(7) 0.093(4) Uani 1 1 d . . . H4A H 0.3268 -0.3141 0.0286 0.111 Uiso 1 1 calc R . . C6A C 0.3858(2) -0.0208(8) 0.1652(4) 0.0603(15) Uani 1 1 d . . . H6A H 0.3768 0.0641 0.1930 0.072 Uiso 1 1 calc R . . C5A C 0.3421(3) -0.1224(10) 0.1082(5) 0.084(2) Uani 1 1 d . . . H5A H 0.3035 -0.1061 0.0969 0.101 Uiso 1 1 calc R . . C7A C 0.5242(3) 0.2185(7) 0.1919(4) 0.0456(14) Uani 1 1 d . . . C8A C 0.5086(3) 0.1934(10) 0.1083(4) 0.0584(16) Uani 1 1 d . . . H8A H 0.4844 0.1049 0.0795 0.070 Uiso 1 1 calc R . . C9A C 0.5286(4) 0.2993(11) 0.0655(5) 0.075(2) Uani 1 1 d . . . H9A H 0.5174 0.2831 0.0080 0.090 Uiso 1 1 calc R . . C10A C 0.5647(3) 0.4270(9) 0.1085(4) 0.0711(18) Uani 1 1 d . . . H10A H 0.5792 0.4962 0.0805 0.085 Uiso 1 1 calc R . . C11A C 0.5796(3) 0.4542(8) 0.1914(4) 0.0697(18) Uani 1 1 d . . . H11A H 0.6034 0.5441 0.2194 0.084 Uiso 1 1 calc R . . C12A C 0.5604(2) 0.3519(9) 0.2347(4) 0.0617(17) Uani 1 1 d . . . H12A H 0.5712 0.3708 0.2920 0.074 Uiso 1 1 calc R . . N N 0.0855(2) 0.3556(8) 0.1174(4) 0.0775(17) Uani 1 1 d . . . F1 F 0.2061(15) 0.7211(18) 0.1559(10) 0.130(6) Uani 0.69 1 d P . . F2 F 0.2793(4) 0.602(3) 0.2488(13) 0.114(5) Uani 0.69 1 d P . . F3 F 0.1990(9) 0.544(3) 0.2354(13) 0.114(7) Uani 0.69 1 d P . . F'1 F 0.259(3) 0.702(6) 0.198(4) 0.140(18) Uani 0.31 1 d P . . F'2 F 0.243(5) 0.524(4) 0.263(2) 0.20(3) Uani 0.31 1 d P . . F'3 F 0.1763(10) 0.656(6) 0.170(4) 0.137(16) Uani 0.31 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Au 0.0410(2) 0.0450(2) 0.0413(2) -0.00192(12) 0.01977(15) -0.00554(11) P 0.0430(10) 0.0470(12) 0.0393(10) 0.000 0.0219(8) 0.000 S1 0.0500(8) 0.0571(9) 0.0596(10) -0.0133(7) 0.0309(7) -0.0159(7) S2 0.0530(8) 0.0718(11) 0.0627(9) -0.0228(8) 0.0310(7) -0.0218(7) C1 0.048(3) 0.041(3) 0.053(3) -0.003(2) 0.030(2) -0.003(2) C2 0.059(3) 0.049(3) 0.050(3) -0.005(3) 0.028(3) -0.006(3) C3 0.057(3) 0.052(4) 0.064(4) -0.004(3) 0.033(3) -0.007(3) C4 0.079(5) 0.061(5) 0.071(5) -0.017(4) 0.040(4) -0.012(4) C1A 0.056(3) 0.057(4) 0.046(3) -0.003(3) 0.031(3) -0.013(3) C2A 0.095(5) 0.085(5) 0.108(6) -0.041(5) 0.078(5) -0.040(5) C3A 0.144(10) 0.114(8) 0.117(8) -0.067(6) 0.103(8) -0.085(7) C4A 0.117(9) 0.098(7) 0.066(5) -0.014(4) 0.044(6) -0.067(6) C6A 0.055(3) 0.057(4) 0.067(4) 0.004(3) 0.025(3) -0.002(3) C5A 0.063(4) 0.079(5) 0.089(5) 0.016(5) 0.016(4) -0.021(4) C7A 0.042(3) 0.054(4) 0.040(3) 0.008(2) 0.018(3) -0.001(2) C8A 0.072(4) 0.058(3) 0.052(4) -0.005(3) 0.035(3) -0.016(3) C9A 0.099(6) 0.083(5) 0.055(4) 0.001(4) 0.046(4) -0.019(5) C10A 0.084(4) 0.068(5) 0.068(4) 0.012(3) 0.040(4) -0.020(3) C11A 0.063(4) 0.063(4) 0.068(4) 0.006(3) 0.018(3) -0.020(3) C12A 0.062(4) 0.067(5) 0.045(3) -0.003(3) 0.015(3) -0.019(3) N 0.069(3) 0.082(5) 0.101(5) -0.021(4) 0.056(3) -0.016(3) F1 0.203(19) 0.060(7) 0.115(9) -0.015(6) 0.063(14) 0.014(9) F2 0.072(4) 0.162(15) 0.101(10) -0.085(8) 0.034(5) -0.026(7) F3 0.148(10) 0.123(14) 0.129(13) -0.066(11) 0.114(10) -0.061(12) F'1 0.22(4) 0.10(2) 0.17(4) -0.09(2) 0.16(3) -0.12(3) F'2 0.44(8) 0.11(3) 0.061(17) 0.008(17) 0.12(4) 0.04(6) F'3 0.089(13) 0.09(2) 0.22(4) -0.10(3) 0.070(18) -0.004(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au S2 2.2848(15) . ? Au S2 2.2848(15) 7 ? Au S1 2.2948(16) 7 ? Au S1 2.2948(16) . ? P C7A 1.781(6) . ? P C7A 1.781(6) 2_655 ? P C1A 1.786(5) . ? P C1A 1.786(5) 2_655 ? S1 C1 1.742(6) . ? S2 C2 1.720(6) . ? C1 C2 1.336(7) . ? C1 C3 1.412(7) . ? C2 C4 1.510(8) . ? C3 N 1.134(6) . ? C4 F'2 1.20(2) . ? C4 F3 1.269(13) . ? C4 F'1 1.27(2) . ? C4 F2 1.279(11) . ? C4 F1 1.299(13) . ? C4 F'3 1.31(2) . ? C1A C6A 1.363(7) . ? C1A C2A 1.382(10) . ? C2A C3A 1.379(12) . ? C3A C4A 1.326(19) . ? C4A C5A 1.375(13) . ? C6A C5A 1.382(9) . ? C7A C8A 1.357(9) . ? C7A C12A 1.397(8) . ? C8A C9A 1.386(11) . ? C9A C10A 1.361(10) . ? C10A C11A 1.352(9) . ? C11A C12A 1.364(9) . ? F1 F'3 1.06(4) . ? F1 F'1 1.22(6) . ? F2 F'1 1.14(5) . ? F2 F'2 1.25(7) . ? F3 F'2 1.02(9) . ? F3 F'3 1.36(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S2 Au S2 180.00(6) . 7 ? S2 Au S1 90.34(5) . 7 ? S2 Au S1 89.66(5) 7 7 ? S2 Au S1 89.66(5) . . ? S2 Au S1 90.34(5) 7 . ? S1 Au S1 180.00(13) 7 . ? C7A P C7A 106.2(4) . 2_655 ? C7A P C1A 111.3(3) . . ? C7A P C1A 110.6(3) 2_655 . ? C7A P C1A 110.6(3) . 2_655 ? C7A P C1A 111.3(3) 2_655 2_655 ? C1A P C1A 106.9(4) . 2_655 ? C1 S1 Au 101.40(18) . . ? C2 S2 Au 102.35(19) . . ? C2 C1 C3 124.2(5) . . ? C2 C1 S1 123.2(4) . . ? C3 C1 S1 112.6(4) . . ? C1 C2 C4 122.4(6) . . ? C1 C2 S2 123.0(5) . . ? C4 C2 S2 114.5(4) . . ? N C3 C1 177.5(7) . . ? F'2 C4 F3 49(4) . . ? F'2 C4 F'1 108(3) . . ? F3 C4 F'1 131.0(13) . . ? F'2 C4 F2 60(4) . . ? F3 C4 F2 105.3(11) . . ? F'1 C4 F2 53(3) . . ? F'2 C4 F1 136(2) . . ? F3 C4 F1 107.2(12) . . ? F'1 C4 F1 57(3) . . ? F2 C4 F1 107.5(12) . . ? F'2 C4 F'3 109(3) . . ? F3 C4 F'3 64(3) . . ? F'1 C4 F'3 100(3) . . ? F2 C4 F'3 136.2(12) . . ? F1 C4 F'3 48(2) . . ? F'2 C4 C2 113.1(17) . . ? F3 C4 C2 114.3(8) . . ? F'1 C4 C2 114.6(13) . . ? F2 C4 C2 111.8(7) . . ? F1 C4 C2 110.3(8) . . ? F'3 C4 C2 111.0(14) . . ? C6A C1A C2A 120.4(6) . . ? C6A C1A P 121.5(5) . . ? C2A C1A P 118.0(5) . . ? C3A C2A C1A 119.1(9) . . ? C4A C3A C2A 120.5(10) . . ? C3A C4A C5A 121.3(8) . . ? C1A C6A C5A 119.3(7) . . ? C4A C5A C6A 119.3(8) . . ? C8A C7A C12A 119.6(6) . . ? C8A C7A P 122.1(5) . . ? C12A C7A P 118.2(5) . . ? C7A C8A C9A 120.3(7) . . ? C10A C9A C8A 119.4(7) . . ? C11A C10A C9A 120.6(6) . . ? C10A C11A C12A 121.0(6) . . ? C11A C12A C7A 119.0(6) . . ? F'3 F1 F'1 121(3) . . ? F'3 F1 C4 67(2) . . ? F'1 F1 C4 60.5(17) . . ? F'1 F2 F'2 113(3) . . ? F'1 F2 C4 63.0(18) . . ? F'2 F2 C4 57(2) . . ? F'2 F3 C4 62(2) . . ? F'2 F3 F'3 118(3) . . ? C4 F3 F'3 59.6(14) . . ? F2 F'1 F1 124(2) . . ? F2 F'1 C4 64.0(18) . . ? F1 F'1 C4 62.9(19) . . ? F3 F'2 C4 69(3) . . ? F3 F'2 F2 126(3) . . ? C4 F'2 F2 63(2) . . ? F1 F'3 C4 65.6(16) . . ? F1 F'3 F3 117(3) . . ? C4 F'3 F3 57(2) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.753 _refine_diff_density_min -1.291 _refine_diff_density_rms 0.355 # Attachment 'B608420F_transTBAAu.cif' data_oj160a _database_code_depnum_ccdc_archive 'CCDC 616051' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'TBA, Au(tfadt)2 ' _chemical_melting_point ? _chemical_formula_moiety 'C16 H36 N, C8 Au F6 N2 S4' _chemical_formula_sum 'C24 H36 Au F6 N3 S4' _chemical_formula_weight 805.76 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.1550(13) _cell_length_b 11.7052(13) _cell_length_c 13.5301(15) _cell_angle_alpha 73.117(13) _cell_angle_beta 78.734(14) _cell_angle_gamma 67.536(13) _cell_volume 1555.1(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 1.95 _cell_measurement_theta_max 25.75 _exptl_crystal_description plate _exptl_crystal_colour 'pale brown' _exptl_crystal_size_max 0.72 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.721 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 796 _exptl_absorpt_coefficient_mu 5.054 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; a grid of 8 x 16 x 8 = 1024 sampling points was used ; _exptl_absorpt_correction_T_min 0.2489 _exptl_absorpt_correction_T_max 0.8603 _exptl_absorpt_correction_T_ave 0.7609 _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS' _diffrn_measurement_method 'Oscillation, phi incr. 1.7 deg' _diffrn_detector_area_resol_mean 6.66 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15016 _diffrn_reflns_av_R_equivalents 0.0641 _diffrn_reflns_av_sigmaI/netI 0.0677 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 25.87 _reflns_number_total 5563 _reflns_number_gt 4285 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'EXPOSE, Stoe-IPDS' _computing_cell_refinement 'CELL, Stoe-IPDS' _computing_data_reduction 'INTEGRATE, Stoe-IPDS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0433P)^2^+1.0976P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment Constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5563 _refine_ls_number_parameters 343 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0606 _refine_ls_R_factor_gt 0.0385 _refine_ls_wR_factor_ref 0.0946 _refine_ls_wR_factor_gt 0.0847 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au Au 0.42940(3) 0.91857(2) 0.14519(2) 0.03128(10) Uani 1 1 d . . . S1 S 0.28159(18) 1.10946(16) 0.06712(14) 0.0393(4) Uani 1 1 d . . . S2 S 0.38064(19) 0.81704(16) 0.04320(14) 0.0387(4) Uani 1 1 d . . . S3 S 0.57832(19) 0.72877(16) 0.22347(14) 0.0405(4) Uani 1 1 d . . . S4 S 0.47783(18) 1.02175(17) 0.24517(15) 0.0398(4) Uani 1 1 d . . . C1 C 0.2224(6) 1.0633(7) -0.0197(5) 0.0343(16) Uani 1 1 d . . . C2 C 0.2619(7) 0.9421(7) -0.0286(5) 0.0374(17) Uani 1 1 d . . . C3 C 0.2041(9) 0.9001(8) -0.0970(6) 0.049(2) Uani 1 1 d . . . C4 C 0.1320(7) 1.1705(7) -0.0831(6) 0.0412(18) Uani 1 1 d . . . C5 C 0.6408(7) 0.7786(6) 0.3063(5) 0.0344(16) Uani 1 1 d . . . C6 C 0.5998(7) 0.8983(7) 0.3153(5) 0.0356(17) Uani 1 1 d . . . C7 C 0.6563(8) 0.9384(7) 0.3872(6) 0.0433(19) Uani 1 1 d . . . C8 C 0.7425(8) 0.6763(8) 0.3637(6) 0.0459(19) Uani 1 1 d . . . C1A C 0.1707(6) 0.5584(6) 0.3091(5) 0.0309(15) Uani 1 1 d . . . H1A1 H 0.0837 0.5775 0.2916 0.037 Uiso 1 1 calc R . . H1A2 H 0.1727 0.5186 0.3827 0.037 Uiso 1 1 calc R . . C2A C 0.1930(7) 0.6828(6) 0.2903(5) 0.0343(15) Uani 1 1 d . . . H2A1 H 0.1866 0.7271 0.2177 0.041 Uiso 1 1 calc R . . H2A2 H 0.2796 0.6665 0.3071 0.041 Uiso 1 1 calc R . . C3A C 0.0914(7) 0.7646(7) 0.3576(7) 0.049(2) Uani 1 1 d . . . H3A1 H 0.0998 0.7197 0.4299 0.058 Uiso 1 1 calc R . . H3A2 H 0.0054 0.7767 0.3422 0.058 Uiso 1 1 calc R . . C4A C 0.1027(9) 0.8945(7) 0.3421(8) 0.061(2) Uani 1 1 d . . . H4A1 H 0.0353 0.9419 0.3858 0.092 Uiso 1 1 calc R . . H4A2 H 0.0936 0.9400 0.2708 0.092 Uiso 1 1 calc R . . H4A3 H 0.1863 0.8834 0.3598 0.092 Uiso 1 1 calc R . . C5A C 0.2352(6) 0.3397(6) 0.2902(5) 0.0334(15) Uani 1 1 d . . . H5A1 H 0.3038 0.2736 0.2616 0.040 Uiso 1 1 calc R . . H5A2 H 0.2370 0.3141 0.3650 0.040 Uiso 1 1 calc R . . C6A C 0.1055(7) 0.3472(6) 0.2652(6) 0.0406(17) Uani 1 1 d . . . H6A1 H 0.1092 0.3525 0.1918 0.049 Uiso 1 1 calc R . . H6A2 H 0.0374 0.4230 0.2809 0.049 Uiso 1 1 calc R . . C7A C 0.0742(8) 0.2283(7) 0.3295(7) 0.052(2) Uani 1 1 d . . . H7A1 H 0.1414 0.1531 0.3121 0.062 Uiso 1 1 calc R . . H7A2 H 0.0742 0.2217 0.4027 0.062 Uiso 1 1 calc R . . C8A C -0.0571(9) 0.2337(8) 0.3097(9) 0.074(3) Uani 1 1 d . . . H8A1 H -0.0740 0.1587 0.3513 0.110 Uiso 1 1 calc R . . H8A2 H -0.0566 0.2381 0.2376 0.110 Uiso 1 1 calc R . . H8A3 H -0.1239 0.3077 0.3276 0.110 Uiso 1 1 calc R . . C9A C 0.4054(6) 0.4349(6) 0.2659(5) 0.0321(15) Uani 1 1 d . . . H9A1 H 0.4260 0.5117 0.2341 0.038 Uiso 1 1 calc R . . H9A2 H 0.4616 0.3706 0.2291 0.038 Uiso 1 1 calc R . . C10A C 0.4384(7) 0.3898(7) 0.3777(5) 0.0366(16) Uani 1 1 d . . . H10A H 0.3845 0.4536 0.4156 0.044 Uiso 1 1 calc R . . H10B H 0.4205 0.3118 0.4105 0.044 Uiso 1 1 calc R . . C11A C 0.5803(7) 0.3668(8) 0.3811(6) 0.0457(19) Uani 1 1 d . . . H11A H 0.5961 0.4466 0.3533 0.055 Uiso 1 1 calc R . . H11B H 0.6335 0.3090 0.3378 0.055 Uiso 1 1 calc R . . C13A C 0.2483(7) 0.5176(6) 0.1352(5) 0.0335(15) Uani 1 1 d . . . H13A H 0.1581 0.5374 0.1255 0.040 Uiso 1 1 calc R . . H13B H 0.2655 0.5969 0.1140 0.040 Uiso 1 1 calc R . . C12A C 0.6201(9) 0.3106(9) 0.4914(7) 0.062(2) Uani 1 1 d . . . H12A H 0.7107 0.2969 0.4908 0.093 Uiso 1 1 calc R . . H12B H 0.6058 0.2310 0.5187 0.093 Uiso 1 1 calc R . . H12C H 0.5689 0.3685 0.5341 0.093 Uiso 1 1 calc R . . F1 F 0.1300(9) 0.9931(6) -0.1623(6) 0.126(3) Uani 1 1 d . . . F2 F 0.1343(6) 0.8285(7) -0.0411(4) 0.089(2) Uani 1 1 d . . . F3 F 0.2937(6) 0.8252(5) -0.1526(4) 0.0709(15) Uani 1 1 d . . . F4 F 0.6116(6) 1.0635(5) 0.3786(4) 0.0704(15) Uani 1 1 d . . . F5 F 0.6293(7) 0.8880(5) 0.4851(4) 0.0833(19) Uani 1 1 d . . . F6 F 0.7835(6) 0.9073(8) 0.3709(6) 0.113(3) Uani 1 1 d . . . N1A N 0.2661(5) 0.4621(5) 0.2501(4) 0.0292(12) Uani 1 1 d . . . N1 N 0.0622(7) 1.2604(6) -0.1311(5) 0.0534(18) Uani 1 1 d . . . N2 N 0.8190(8) 0.5958(8) 0.4086(6) 0.070(2) Uani 1 1 d . . . C14A C 0.3345(7) 0.4320(7) 0.0650(5) 0.0408(17) Uani 1 1 d . . . H14A H 0.3212 0.3508 0.0876 0.049 Uiso 1 1 calc R . . H14B H 0.4251 0.4165 0.0705 0.049 Uiso 1 1 calc R . . C15A C 0.3055(8) 0.4909(8) -0.0478(6) 0.0462(19) Uani 1 1 d . . . H15A H 0.3108 0.5755 -0.0680 0.055 Uiso 1 1 calc R . . H15B H 0.3716 0.4401 -0.0912 0.055 Uiso 1 1 calc R . . C16A C 0.1724(9) 0.5000(10) -0.0671(6) 0.065(3) Uani 1 1 d . . . H16A H 0.1593 0.5383 -0.1390 0.098 Uiso 1 1 calc R . . H16B H 0.1064 0.5513 -0.0251 0.098 Uiso 1 1 calc R . . H16C H 0.1673 0.4163 -0.0493 0.098 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Au 0.03012(15) 0.02727(14) 0.03186(14) -0.00131(9) -0.00267(9) -0.00935(10) S1 0.0367(10) 0.0270(8) 0.0478(10) -0.0022(8) -0.0159(8) -0.0034(8) S2 0.0450(11) 0.0289(8) 0.0397(9) -0.0027(8) -0.0100(8) -0.0115(8) S3 0.0467(11) 0.0251(8) 0.0399(9) -0.0034(7) -0.0128(8) -0.0010(8) S4 0.0362(10) 0.0313(9) 0.0503(10) -0.0102(8) -0.0113(8) -0.0060(8) C1 0.025(4) 0.040(4) 0.032(3) 0.003(3) -0.002(3) -0.014(3) C2 0.040(4) 0.044(4) 0.030(3) -0.003(3) -0.004(3) -0.020(4) C3 0.059(6) 0.050(5) 0.041(4) -0.008(4) -0.012(4) -0.020(4) C4 0.033(4) 0.045(4) 0.042(4) -0.003(4) -0.002(3) -0.016(4) C5 0.029(4) 0.035(4) 0.032(3) -0.004(3) -0.001(3) -0.006(3) C6 0.029(4) 0.042(4) 0.031(3) -0.003(3) -0.005(3) -0.011(3) C7 0.037(4) 0.047(4) 0.040(4) -0.011(4) -0.001(3) -0.009(4) C8 0.045(5) 0.045(4) 0.036(4) -0.005(4) -0.005(3) -0.006(4) C1A 0.026(3) 0.029(3) 0.036(3) -0.008(3) -0.003(3) -0.008(3) C2A 0.033(4) 0.028(3) 0.041(4) -0.008(3) -0.007(3) -0.008(3) C3A 0.032(4) 0.040(4) 0.073(5) -0.025(4) 0.002(4) -0.006(3) C4A 0.060(6) 0.034(4) 0.090(7) -0.024(4) -0.013(5) -0.007(4) C5A 0.028(4) 0.024(3) 0.043(4) -0.004(3) -0.006(3) -0.006(3) C6A 0.032(4) 0.033(4) 0.060(4) -0.010(3) -0.011(3) -0.013(3) C7A 0.038(4) 0.031(4) 0.084(6) -0.008(4) -0.008(4) -0.014(4) C8A 0.040(5) 0.043(5) 0.137(9) -0.015(5) -0.005(5) -0.020(4) C9A 0.021(3) 0.033(3) 0.043(4) -0.010(3) -0.005(3) -0.008(3) C10A 0.029(4) 0.040(4) 0.041(4) -0.005(3) -0.009(3) -0.013(3) C11A 0.033(4) 0.052(5) 0.051(4) -0.009(4) -0.009(3) -0.014(4) C13A 0.040(4) 0.031(3) 0.033(3) -0.004(3) -0.008(3) -0.016(3) C12A 0.051(5) 0.080(6) 0.065(5) -0.015(5) -0.016(4) -0.030(5) F1 0.179(8) 0.063(4) 0.148(6) -0.020(4) -0.134(6) -0.001(4) F2 0.085(4) 0.146(6) 0.080(4) -0.038(4) 0.012(3) -0.089(4) F3 0.081(4) 0.087(4) 0.066(3) -0.036(3) 0.003(3) -0.043(3) F4 0.100(4) 0.055(3) 0.070(3) -0.015(3) -0.026(3) -0.033(3) F5 0.142(6) 0.078(4) 0.044(3) -0.001(3) -0.024(3) -0.055(4) F6 0.037(3) 0.175(7) 0.157(6) -0.106(6) -0.003(4) -0.023(4) N1A 0.026(3) 0.023(3) 0.036(3) -0.002(2) -0.007(2) -0.006(2) N1 0.044(4) 0.047(4) 0.060(4) -0.001(3) -0.016(3) -0.009(3) N2 0.058(5) 0.069(5) 0.054(4) 0.002(4) -0.013(4) 0.001(4) C14A 0.034(4) 0.040(4) 0.048(4) -0.014(3) -0.012(3) -0.007(3) C15A 0.054(5) 0.048(4) 0.039(4) -0.015(4) -0.007(3) -0.016(4) C16A 0.069(7) 0.079(6) 0.048(5) -0.018(5) -0.017(4) -0.017(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au S4 2.305(2) . ? Au S3 2.3060(18) . ? Au S1 2.3068(18) . ? Au S2 2.314(2) . ? S1 C1 1.747(8) . ? S2 C2 1.743(7) . ? S3 C5 1.755(8) . ? S4 C6 1.745(7) . ? C1 C2 1.350(10) . ? C1 C4 1.440(10) . ? C2 C3 1.501(11) . ? C3 F1 1.299(10) . ? C3 F3 1.325(10) . ? C3 F2 1.334(9) . ? C4 N1 1.145(9) . ? C5 C6 1.332(10) . ? C5 C8 1.446(10) . ? C6 C7 1.516(11) . ? C7 F5 1.310(8) . ? C7 F6 1.313(9) . ? C7 F4 1.331(9) . ? C8 N2 1.114(10) . ? C1A C2A 1.512(8) . ? C1A N1A 1.521(8) . ? C2A C3A 1.518(10) . ? C3A C4A 1.524(10) . ? C5A C6A 1.515(9) . ? C5A N1A 1.522(7) . ? C6A C7A 1.538(9) . ? C7A C8A 1.514(12) . ? C9A N1A 1.508(8) . ? C9A C10A 1.519(9) . ? C10A C11A 1.509(10) . ? C11A C12A 1.523(11) . ? C13A C14A 1.514(10) . ? C13A N1A 1.521(8) . ? C14A C15A 1.524(10) . ? C15A C16A 1.516(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S4 Au S3 89.95(7) . . ? S4 Au S1 89.58(7) . . ? S3 Au S1 179.46(8) . . ? S4 Au S2 179.33(6) . . ? S3 Au S2 90.57(7) . . ? S1 Au S2 89.90(7) . . ? C1 S1 Au 101.7(2) . . ? C2 S2 Au 101.8(3) . . ? C5 S3 Au 101.3(2) . . ? C6 S4 Au 101.9(3) . . ? C2 C1 C4 124.6(7) . . ? C2 C1 S1 123.5(5) . . ? C4 C1 S1 111.8(5) . . ? C1 C2 C3 123.8(7) . . ? C1 C2 S2 123.0(6) . . ? C3 C2 S2 113.2(6) . . ? F1 C3 F3 106.5(7) . . ? F1 C3 F2 107.8(8) . . ? F3 C3 F2 103.7(7) . . ? F1 C3 C2 114.1(7) . . ? F3 C3 C2 112.7(7) . . ? F2 C3 C2 111.4(6) . . ? N1 C4 C1 175.9(9) . . ? C6 C5 C8 123.3(7) . . ? C6 C5 S3 123.7(6) . . ? C8 C5 S3 113.0(6) . . ? C5 C6 C7 122.4(7) . . ? C5 C6 S4 123.1(6) . . ? C7 C6 S4 114.5(5) . . ? F5 C7 F6 107.1(7) . . ? F5 C7 F4 105.5(7) . . ? F6 C7 F4 104.8(7) . . ? F5 C7 C6 112.0(6) . . ? F6 C7 C6 113.2(7) . . ? F4 C7 C6 113.7(6) . . ? N2 C8 C5 178.4(10) . . ? C2A C1A N1A 116.8(5) . . ? C1A C2A C3A 109.2(5) . . ? C2A C3A C4A 113.4(6) . . ? C6A C5A N1A 115.5(5) . . ? C5A C6A C7A 109.7(6) . . ? C8A C7A C6A 111.5(7) . . ? N1A C9A C10A 116.0(5) . . ? C11A C10A C9A 110.0(5) . . ? C10A C11A C12A 111.6(6) . . ? C14A C13A N1A 114.9(5) . . ? C9A N1A C1A 111.8(5) . . ? C9A N1A C13A 108.6(5) . . ? C1A N1A C13A 107.9(5) . . ? C9A N1A C5A 109.3(5) . . ? C1A N1A C5A 107.7(5) . . ? C13A N1A C5A 111.5(5) . . ? C13A C14A C15A 111.7(6) . . ? C16A C15A C14A 113.1(6) . . ? _diffrn_measured_fraction_theta_max 0.922 _diffrn_reflns_theta_full 25.87 _diffrn_measured_fraction_theta_full 0.922 _refine_diff_density_max 1.147 _refine_diff_density_min -1.739 _refine_diff_density_rms 0.163